CN113278250A - Ti3SiC2Method for preparing ceramic reinforced composite material - Google Patents

Ti3SiC2Method for preparing ceramic reinforced composite material Download PDF

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CN113278250A
CN113278250A CN202110343433.7A CN202110343433A CN113278250A CN 113278250 A CN113278250 A CN 113278250A CN 202110343433 A CN202110343433 A CN 202110343433A CN 113278250 A CN113278250 A CN 113278250A
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composite material
temperature reaction
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陈梓山
胡淼
陈雨
张展
张颖
李欣
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Shanghai Lingyun Industrial Technology Co ltd
Shanghai Lingyun Industrial Technology Co ltd Lingyun Automobile Technology Branch
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • C04B35/5615—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium silicon carbides
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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Abstract

Ti3SiC2The preparation method of the ceramic reinforced composite material is chemical vapor coprecipitationDeposition method, using methyltrichlorosilane and titanium tetrachloride to deposit Ti on the surface of fiber3SiC2Layer, the deposition process being carried out in a high temperature reactor system, containing Ti3SiC2The fibers of the layer are then compounded with a resin to obtain Ti3SiC2A ceramic reinforced composite material. The method of the invention is not easy to introduce impurities in the codeposition process, and Ti3SiC2The ceramic layer is uniformly distributed, the thickness can be accurately controlled, and the comprehensive mechanical property of the material after the fiber and the resin are compounded is improved.

Description

Ti3SiC2Method for preparing ceramic reinforced composite material
Technical Field
The invention relates to a preparation method of a ceramic reinforced composite material, in particular to Ti3SiC2A method for preparing a ceramic reinforced composite material.
Background
The fiber reinforced resin matrix composite material has the advantages of light weight, high strength, corrosion resistance and the like, and the fiber/resin interface of the fiber reinforced resin matrix composite material has obvious influence on the mechanical property of the composite material. Ti3SiC2The (titanium silicon carbide) is a layered ceramic material, has the characteristics of metal, has better ductility at normal temperature, and has high yield and high stability of ceramic. Ti3SiC2After the carbon fiber is compounded, the mechanical property of the material is obviously improved. At present, Ti3SiC2The carbon fiber compounding method is mainly Physical Vapor Deposition (PVD), in-situ reaction synthesis, hot-pressing sintering molding and other processes, wherein the in-situ reaction and hot-pressing sintering processes are suitable for bulk Ti3SiC2The PVD method is suitable for preparing the thin film, and the PVD method is used for preparing Ti3SiC2The efficiency of (2) is low, and the subsidiary formation phase is more. In addition, the prior methods all adopt SiC fibers compounded with Ti, because the SiC fibers are in a solid-phase bulk material state and TThe reaction rate of i atoms is very slow and even impossible.
Disclosure of Invention
The invention provides Ti for overcoming the defects of the prior art3SiC2The preparation method of the ceramic reinforced composite material utilizes a chemical vapor codeposition method to ensure that the methyltrichlorosilane and the titanium tetrachloride quickly deposit Ti on the surface of the fiber3SiC2A ceramic layer, which is less prone to impurity introduction during codeposition, and Ti3SiC2The layers are uniformly distributed, and the comprehensive mechanical property of the material compounded by the fibers and the resin is improved.
The technical scheme adopted by the invention for solving the technical problems is as follows:
ti3SiC2The preparation method of the ceramic reinforced composite material is a chemical vapor codeposition method, and Ti is deposited on the surface of the fiber by utilizing methyltrichlorosilane and titanium tetrachloride3SiC2A ceramic layer, the deposition process being carried out in a high temperature reaction furnace system, containing Ti3Compounding the fiber of the Si ceramic layer with resin to obtain Ti3SiC2The preparation method of the ceramic reinforced composite material comprises the following steps:
a. adding methyl trichlorosilane and titanium tetrachloride into two containers respectively, and heating in water bath respectively;
b. cleaning the surface of the fiber, suspending the fiber in a high-temperature reaction furnace, vacuumizing the high-temperature reaction furnace until the air pressure in the furnace chamber is not higher than 1000Pa, then filling argon as protective atmosphere to normal pressure, and closing an argon bottle valve; simultaneously, the furnace is heated to 1100-1350 ℃ at the heating rate of 5-20 ℃/min and then is insulated;
c. opening the valve of the argon bottle again, filling argon into the high-temperature reaction furnace, simultaneously opening the vacuum pump, and adjusting the pressure in the high-temperature reaction furnace to 5000-;
d. hydrogen is used as carrier gas and diluent gas, the methyl trichlorosilane and titanium tetrachloride which are heated in a water bath are introduced into a high-temperature reaction furnace cavity, the methyl trichlorosilane and the titanium tetrachloride react and codeposit on the surface of the fiber, after the reaction is finished, argon is kept to be filled and a vacuum pump is started, and Ti is obtained after cooling3SiC2Fibers of the layer;
e. prepared Ti-containing3SiC2The fibers of the layer are mixed with a resin to obtain Ti3SiC2A ceramic reinforced composite.
The above Ti3SiC2In the step a, the water bath heating temperature of the methyltrichlorosilane is 65-80 ℃, and the water bath heating temperature of the titanium tetrachloride is 10-25 ℃.
The above Ti3SiC2In the step c, the reaction codeposition time is 20-80min, the codeposition rate is 90-100nm/min, and the deposition thickness is 10nm-100 mu m.
The above Ti3SiC2In the step d, the resin is thermoplastic resin or thermosetting resin; when the resin is a thermoplastic resin, Ti is contained3SiC2Mixing the fiber of the layer with resin, and preparing the composite material by adopting a blending injection molding process; when the resin is a thermosetting resin, Ti is contained3SiC2The fibers of the layers are mixed with the resin and the composite material is prepared by adopting a vacuum infusion process.
The above Ti3SiC2The preparation method of the ceramic reinforced composite material comprises the following specific steps of: prepared Ti-containing3SiC2Laying the fiber of the layer into a die cavity pre-sprayed with a release agent, adding resin into the die cavity to perform vacuum infiltration and impregnation on the fiber in the die cavity, curing for 2h at 75 ℃, and demolding to obtain Ti3SiC2A ceramic reinforced composite.
The above Ti3SiC2The preparation method of the ceramic reinforced composite material comprises the steps that the high-temperature reaction furnace system comprises a first water bath heater, a second water bath heater, a high-temperature reaction furnace, an argon bottle, a first hydrogen bottle and a second hydrogen bottle, methyl trichlorosilane and titanium tetrachloride are added into closed containers, the two closed containers are respectively placed in the first water bath heater and the second water bath heater, and the first hydrogen bottle and the second hydrogen bottle are respectively filled with tetrachloro through a first flowmeter and a second flowmeterThe device comprises a high-temperature reaction furnace, a titanium tank, a high-temperature reaction furnace, a hydrogen tank, a first water bath heater, a second water bath heater, an argon bottle, a vacuum pump, a pipeline and a pipeline, a high-are connected with a high-to high-to be connected with a high-to be connected with high-temperature reaction furnace are connected with high-to high-are connected with high-temperature reaction furnace, the high-temperature reaction furnace are connected with high-temperature reaction furnace.
The above Ti3SiC2The preparation method of the ceramic reinforced composite material is characterized in that a filter is arranged between the high-temperature reaction furnace and the vacuum pump.
The above Ti3SiC2The preparation method of the ceramic reinforced composite material comprises the step of preparing a ceramic reinforced composite material, wherein the fiber is carbon fiber or basalt fiber.
The invention has the beneficial effects that:
the invention utilizes the chemical vapor codeposition method to rapidly deposit Ti on the surface of the fiber by titanium tetrachloride and methyltrichlorosilane3SiC2Layer, the deposition process can accurately control Ti3SiC2The thickness of the layer ensures that the composite material has excellent mechanical properties; the preparation method of the invention can prepare Ti on the surface of the fiber3SiC2Higher purity, less possibility of introducing impurities, and Ti3SiC2The ceramic layer is more uniformly distributed on the surface of the fiber, so that the surface roughness of the fiber is uniform, the mechanical meshing effect between the fiber and the vertical fiber is effectively improved, the interface strength is improved, and the mechanical property of the composite material is improved.
Drawings
FIG. 1 is a schematic diagram of the reaction system of the present invention;
FIG. 2 shows Ti deposition3SiC2Scanning electron microscopy of the fiber surface of the layer;
FIG. 3 shows Ti deposition3SiC2Energy spectrum of the fibers of the layer.
In the figure: 1. a first water bath heater; 2. a second water bath heater; 3. a high-temperature reaction furnace; 4. an argon bottle; 5. a first hydrogen cylinder; 6. a second hydrogen cylinder; 7. a first flow meter; 8. a second flow meter; 9. a barometer; 10. a vacuum pump; 11. a filter; 12. and a third flow meter.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention utilizes a chemical vapor codeposition method to deposit Ti on the surface of a fiber by adopting titanium tetrachloride and methyltrichlorosilane3SiC2A layer, the deposition reaction formula being:
CH3Cl3Si＝SiC+3HCl
2SiC+3TiCl4+5H2＝Ti3SiC2+SiCl2+10HCl
in the vapor codeposition reaction process, SiC and Ti are in atomic or molecular states, the reaction is active, the reaction can be rapidly carried out, and the thickness of a deposition layer can be accurately controlled.
Deposition of Ti on the surface of the fibres3SiC2After coating, the surface roughness of the fiber is increased, the mechanical meshing effect of the fiber and the resin is effectively improved, and the interface strength is improved, so that the mechanical property of the composite material is improved; on the other hand, by introducing Ti excellent in ductility3SiC2The coating can obviously adjust the residual stress of the fiber and resin interface, relieve the phenomenon of material failure caused by stress concentration of the interface area and be beneficial to the improvement of the toughness of the material.
Control of Ti3SiC2The layer is deposited to a thickness of 10nm to 100 μm, Ti3SiC2The thickness of the layer is too small to function as an interface transition, but Ti3SiC2If the thickness of the layer is too large, the interface of the material is weakened and delaminated, and the mechanical property of the material is reduced.
Example 1
And (3) ultrasonically cleaning the carbon fiber fabric by using absolute ethyl alcohol, and drying the carbon fiber fabric in an oven for later use.
Methyltrichlorosilane and titanium tetrachloride were placed in the closed container shown in fig. 1, respectively, and the methyltrichlorosilane was heated to 70 ℃ by the first water bath heater 1, and the temperature of the titanium tetrachloride was maintained at 20 ℃ by the second water bath heater 2.
Suspending the dried carbon fiber fabric in a high-temperature reaction furnace 3, closing the furnace door, vacuumizing to 300Pa, and then filling argon to normal pressure. Then, the furnace temperature is increased to 1200 ℃ at the heating rate of 8 ℃/min, and the temperature is kept for 15 min.
And opening an argon valve, controlling the flow of argon through a third flowmeter 12, filling the argon into the high-temperature reaction furnace 3 at the speed of 2L/min, simultaneously opening a vacuum pump 10, and adjusting the pressure in the furnace to be 5000 Pa. After the pressure in the high-temperature reaction furnace chamber is stabilized, valves for controlling methyl trichlorosilane and titanium tetrachloride are respectively opened, methyl trichlorosilane is loaded into the high-temperature reaction furnace chamber through hydrogen at the flow rate of 1.5L/min by a first flow meter 7, and titanium tetrachloride is loaded into the high-temperature reaction furnace chamber through hydrogen at the flow rate of 0.8L/min by a second flow meter 8. After the methyl trichlorosilane and the titanium tetrachloride are deposited and react on the surface of the carbon fiber for 30min, the valves for controlling the methyl trichlorosilane and the titanium tetrachloride are closed, argon is kept to be filled and the vacuum pump is started, meanwhile, the heating power supply of the high-temperature reaction furnace is closed, the carbon fiber fabric in the furnace is taken out after the furnace is cooled to the room temperature.
Preparing the surface with Ti3SiC2The carbon fiber fabric is placed in a mold, and epoxy resin is introduced into the mold by adopting a vacuum infusion process, and the specific process comprises the following steps: will be prepared with Ti3SiC2Spreading the coated fiber braided fabric (fiber preformed body) into a mold cavity which is pre-sprayed with a release agent, sealing by using a vacuum bag film, forming negative pressure by vacuumizing to promote epoxy resin in a resin barrel to flow into the mold cavity to realize permeation and impregnation of fibers in the mold, heating to 75 ℃ and curing to prepare Ti3SiC2A ceramic reinforced carbon fiber/epoxy composite.
Ti3SiC2Ceramic reinforced carbon fiber/epoxy resin composite material and Ti-free material3SiC2The mechanical properties of the ceramic reinforced carbon fiber/epoxy composite are compared in table 1 below. As can be seen from Table 1, Ti prepared by the process of the present invention3SiC2Compared with the mechanical property of the carbon fiber/epoxy resin composite material without Ti3SiC2The mechanical property of the ceramic reinforced carbon fiber/epoxy resin composite material is obviously improved.
TABLE 1 Presence or absence of Ti3SiC2Mechanical property comparison of ceramic-reinforced carbon fiber/epoxy resin composite material
Figure BDA0002999949340000051
Example 2
And (3) ultrasonically cleaning the carbon fiber fabric by using absolute ethyl alcohol, and drying the carbon fiber fabric in an oven for later use.
Methyltrichlorosilane and titanium tetrachloride were placed in the closed container shown in fig. 1, respectively, and the methyltrichlorosilane was heated to 70 ℃ by the first water bath heater 1, and the temperature of the titanium tetrachloride was maintained at 25 ℃ by the second water bath heater 2.
Suspending the dried carbon fiber fabric in a high-temperature reaction furnace 3, closing the furnace door, vacuumizing to 500Pa, and then filling argon to normal pressure. Then, the furnace temperature is increased to 1350 ℃ at the temperature increasing rate of 10 ℃/min, and the temperature is kept for 15 min.
And opening an argon valve, controlling the flow of argon through a third flowmeter 12, filling the argon into the high-temperature reaction furnace 3 at the speed of 2.5L/min, simultaneously opening a vacuum pump 10, and adjusting the pressure in the furnace to 5500 Pa. After the pressure in the high-temperature reaction furnace chamber is stabilized, valves for controlling methyl trichlorosilane and titanium tetrachloride are respectively opened, methyl trichlorosilane is loaded into the high-temperature reaction furnace chamber through hydrogen at the flow rate of 1.8L/min by a first flow meter 7, and titanium tetrachloride is loaded into the high-temperature reaction furnace chamber through hydrogen at the flow rate of 0.9L/min by a second flow meter 8. After the methyl trichlorosilane and the titanium tetrachloride are deposited and react on the surface of the carbon fiber for 20min, the valves for controlling the methyl trichlorosilane and the titanium tetrachloride are closed, argon is kept to be filled and the vacuum pump is started to be started, meanwhile, the heating power supply of the high-temperature reaction furnace is closed, the carbon fiber fabric in the furnace is taken out after the furnace is cooled to the room temperature.
Preparing the surface with Ti3SiC2The carbon fiber is chopped into fiber sections with the diameter of about 25mm, and the chopped carbon fiber and polyamide are mixed by a screw extruder and then injectedMolding to obtain Ti3SiC2A ceramic reinforced carbon fiber/polyamide composite material.
Ti3SiC2Ceramic reinforced carbon fiber/polyamide composite material and non-used Ti3SiC2The mechanical properties of the ceramic reinforced carbon fiber/polyamide composite material are compared in table 2 below.
TABLE 2 Presence or absence of Ti3SiC2Mechanical property comparison of ceramic-reinforced carbon fiber/polyamide composite material
Figure BDA0002999949340000061
To deposit Ti by the method of the invention3SiC2The fiber surface morphology of the ceramic layer was subjected to scanning electron microscope testing and energy spectrum analysis, and the test results are shown in fig. 2 and 3. As can be seen by combining the energy spectrum analysis of FIG. 2 and FIG. 3, after the chemical vapor co-deposition, a layer of rugged Ti is obtained on the surface of the carbon fiber3SiC2A ceramic layer. On one hand, the rough surface of the ceramic layer effectively improves the mechanical meshing effect of the fiber/resin interface and improves the interface strength. On the other hand, the ceramic layer forms a plastic transition layer on the surface of the fiber, so that stress concentration in the stress process is effectively relieved.

Claims (8)

1. Ti3SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: the method is a chemical vapor codeposition method, and Ti is deposited on the surface of the fiber by utilizing methyltrichlorosilane and titanium tetrachloride3SiC2A ceramic layer, the deposition process being carried out in a high temperature reaction furnace system, containing Ti3SiC2Compounding the fiber of the ceramic layer with resin to obtain Ti3SiC2The preparation method of the ceramic reinforced composite material comprises the following steps:
a. adding methyl trichlorosilane and titanium tetrachloride into two containers respectively, and heating in water bath respectively;
b. cleaning the surface of the fiber, suspending the fiber in a high-temperature reaction furnace, vacuumizing the high-temperature reaction furnace until the air pressure in the furnace chamber is not higher than 1000Pa, then filling argon as protective atmosphere to normal pressure, and closing an argon bottle valve; simultaneously, the furnace is heated to 1100-1350 ℃ at the heating rate of 5-20 ℃/min and then is insulated;
c. opening the valve of the argon bottle again, filling argon into the high-temperature reaction furnace, simultaneously opening the vacuum pump, and adjusting the pressure in the high-temperature reaction furnace to 5000-;
d. hydrogen is used as carrier gas and diluent gas, the methyl trichlorosilane and titanium tetrachloride which are heated in a water bath are introduced into a high-temperature reaction furnace cavity, the methyl trichlorosilane and the titanium tetrachloride react and codeposit on the surface of the fiber, after the reaction is finished, argon is kept to be filled and a vacuum pump is started, and Ti is obtained after cooling3SiC2Fibers of the layer;
e. prepared Ti-containing3SiC2The fibers of the layer are mixed with a resin to obtain Ti3SiC2A ceramic reinforced composite.
2. The Ti of claim 13SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: in the step a, the water bath heating temperature of the methyltrichlorosilane is 65-80 ℃, and the water bath heating temperature of the titanium tetrachloride is 10-25 ℃.
3. The Ti of claim 23SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: in the step c, the reaction codeposition time is 20-80min, the codeposition rate is 90-100nm/min, and the deposition thickness is 10nm-100 mu m.
4. The Ti of claim 33SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: in the step d, the resin is thermoplastic resin or thermosetting resin; when the resin is a thermoplastic resin, Ti is contained3SiC2Mixing the fiber of the layer with resin, and preparing the composite material by adopting a blending injection molding process; when the resin is a thermosetting resin, Ti is contained3SiC2Fibres and resins of the layersThe composite material is prepared by adopting a vacuum infusion process.
5. The Ti of claim 43SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: the vacuum infusion process specifically comprises the following steps: prepared Ti-containing3SiC2Laying the fiber of the layer into a die cavity pre-sprayed with a release agent, adding resin into the die cavity to perform vacuum infiltration and impregnation on the fiber in the die cavity, curing for 2h at 75 ℃, and demolding to obtain Ti3SiC2A ceramic reinforced composite.
6. The Ti of claim 53SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: the high-temperature reaction furnace system comprises a first water bath heater (1), a second water bath heater (2), a high-temperature reaction furnace (3), an argon bottle (4), a first hydrogen bottle (5) and a second hydrogen bottle (6), wherein methyltrichlorosilane and titanium tetrachloride are added into closed containers, the two closed containers are respectively placed in the first water bath heater (1) and the second water bath heater (2), the first hydrogen bottle (5) and the second hydrogen bottle (6) are respectively communicated with the closed containers filled with methyltrichlorosilane and titanium tetrachloride through a first flowmeter (7) and a second flowmeter (8), the two closed containers are respectively connected with the high-temperature reaction furnace (3) through pipelines, hydrogen respectively loads the titanium tetrachloride and the methyltrichlorosilane into the high-temperature reaction furnace for reaction and deposition, the argon bottle (4) is connected with the high-temperature reaction furnace (3) through a third flowmeter (12), the high-temperature reaction furnace (3) is provided with a barometer (9) and is connected with a vacuum pump (10), and the first water bath heater (1), the second water bath heater (2), the argon bottle (4) and the vacuum pump (10) are respectively provided with a switch valve on a connecting pipeline of the high-temperature reaction furnace (3).
7. The Ti of claim 63SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: the high-temperature reaction furnace (3) and theA filter (11) is also arranged between the vacuum pumps (10).
8. The Ti of claim 73SiC2The preparation method of the ceramic reinforced composite material is characterized by comprising the following steps: the fibers are carbon fibers or basalt fibers.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114315394A (en) * 2021-12-21 2022-04-12 西北工业大学 By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4598024A (en) * 1984-09-28 1986-07-01 The United States Of America As Represented By The United States Department Of Energy Dispersion toughened ceramic composites and method for making same
US4882370A (en) * 1988-01-27 1989-11-21 Minnesota Mining And Manufacturing Company Fiber reinforced composites with improved glass transition temperatures
FR2675141A1 (en) * 1991-04-09 1992-10-16 Europ Propulsion Composite material with a ceramic matrix with lamellar interphase between refractory reinforcing fibres and matrix, and process for its manufacture
US6143376A (en) * 1998-06-27 2000-11-07 Daimlerchrysler Method for manufacturing coated short fibers
US6506483B1 (en) * 2000-04-28 2003-01-14 Technology Assessment & Transfer, Inc. Ceramic fiber debond coatings
CN102617985A (en) * 2012-03-31 2012-08-01 武汉理工大学 Hybrid reinforced epoxy resin-based piezoelectric damping composite material and preparation method thereof
CN103910532A (en) * 2013-01-05 2014-07-09 中国科学院宁波材料技术与工程研究所 Coating inorganic fiber toughened MAX phase ceramic composite material, preparation method and uses thereof
CN105541412A (en) * 2016-01-27 2016-05-04 南京工程学院 Preparation method of SiC nanowire-toughened SiC ceramic coating on surface of C/C composite
CN108409347A (en) * 2018-03-09 2018-08-17 中国航发北京航空材料研究院 A kind of in-situ preparation Ti3SiC2The preparation method of phase ceramics of silicon carbide toughened based composites
CN110272611A (en) * 2018-03-14 2019-09-24 中国科学院深圳先进技术研究院 A kind of preparation method of Heat Conduction Material
CN110911705A (en) * 2019-11-20 2020-03-24 上海大学 Ti on fuel cell composite bipolar plate3SiC2Method for producing a coating
CN112479718A (en) * 2020-11-20 2021-03-12 航天特种材料及工艺技术研究所 Ti3SiC2MAX phase interface layer modified SiC/SiC composite material and preparation method thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4598024A (en) * 1984-09-28 1986-07-01 The United States Of America As Represented By The United States Department Of Energy Dispersion toughened ceramic composites and method for making same
US4882370A (en) * 1988-01-27 1989-11-21 Minnesota Mining And Manufacturing Company Fiber reinforced composites with improved glass transition temperatures
FR2675141A1 (en) * 1991-04-09 1992-10-16 Europ Propulsion Composite material with a ceramic matrix with lamellar interphase between refractory reinforcing fibres and matrix, and process for its manufacture
US6143376A (en) * 1998-06-27 2000-11-07 Daimlerchrysler Method for manufacturing coated short fibers
US6506483B1 (en) * 2000-04-28 2003-01-14 Technology Assessment & Transfer, Inc. Ceramic fiber debond coatings
CN102617985A (en) * 2012-03-31 2012-08-01 武汉理工大学 Hybrid reinforced epoxy resin-based piezoelectric damping composite material and preparation method thereof
CN103910532A (en) * 2013-01-05 2014-07-09 中国科学院宁波材料技术与工程研究所 Coating inorganic fiber toughened MAX phase ceramic composite material, preparation method and uses thereof
CN105541412A (en) * 2016-01-27 2016-05-04 南京工程学院 Preparation method of SiC nanowire-toughened SiC ceramic coating on surface of C/C composite
CN108409347A (en) * 2018-03-09 2018-08-17 中国航发北京航空材料研究院 A kind of in-situ preparation Ti3SiC2The preparation method of phase ceramics of silicon carbide toughened based composites
CN110272611A (en) * 2018-03-14 2019-09-24 中国科学院深圳先进技术研究院 A kind of preparation method of Heat Conduction Material
CN110911705A (en) * 2019-11-20 2020-03-24 上海大学 Ti on fuel cell composite bipolar plate3SiC2Method for producing a coating
CN112479718A (en) * 2020-11-20 2021-03-12 航天特种材料及工艺技术研究所 Ti3SiC2MAX phase interface layer modified SiC/SiC composite material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱锡 等编著, 国防工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114315394A (en) * 2021-12-21 2022-04-12 西北工业大学 By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material
CN114315394B (en) * 2021-12-21 2023-03-10 西北工业大学 By using Ti 3 SiC 2 Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material

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Application publication date: 20210820